DE10342828A1 - High purity pyrogenic silica - Google Patents

High purity pyrogenic silica Download PDF

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Publication number
DE10342828A1
DE10342828A1 DE10342828A DE10342828A DE10342828A1 DE 10342828 A1 DE10342828 A1 DE 10342828A1 DE 10342828 A DE10342828 A DE 10342828A DE 10342828 A DE10342828 A DE 10342828A DE 10342828 A1 DE10342828 A1 DE 10342828A1
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Prior art keywords
silica
high purity
silicon tetrachloride
purity
metals
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German (de)
Inventor
Hauke Dr. Mobile Jacobsen
Monika Dr. Oswald
Kai Dr. Schumacher
Martin Dr. Mörters
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Evonik Operations GmbH
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Degussa GmbH
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Priority to DE10342828A priority Critical patent/DE10342828A1/en
Priority to JP2006526581A priority patent/JP4903045B2/en
Priority to PCT/EP2004/010335 priority patent/WO2005026068A2/en
Priority to CNA2004800268452A priority patent/CN1863733A/en
Priority to KR1020067005468A priority patent/KR100789124B1/en
Priority to EP04786950A priority patent/EP1663888A2/en
Priority to US10/571,332 priority patent/US20070003770A1/en
Publication of DE10342828A1 publication Critical patent/DE10342828A1/en
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/02—Pretreated ingredients
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/02—Pure silica glass, e.g. pure fused quartz
    • C03B2201/03—Impurity concentration specified
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

Abstract

Hochreines, pyrogen hergestelltes Siliciumdioxid mit Metallgehalten von kleiner 0,2 mug/g wird hergestellt, indem man ein Siliciumtetrachlorid mit Metallgehalten kleiner 30 ppb mittels Flammenhydrolyse umsetzt. DOLLAR A Das Siliziumdioxid kann zur Herstellung von hochreinen Gläsern mittels des Sol-Gel-Verfahrens eingesetzt werden.High purity fumed silica with metal contents of less than 0.2 mug / g is prepared by reacting a silicon tetrachloride with metal contents below 30 ppb by flame hydrolysis. DOLLAR A The silica can be used to produce high purity glasses by the sol-gel method.

Description

Die Erfindung betrifft ein hochreines, pyrogen hergestelltes Siliciumdioxid, ein Verfahren zu seiner Herstellung sowie seine Verwendung.The This invention relates to a high purity pyrogenic silica, a method for its production and its use.

Kieselglas kann vorteilhaft für viele Einsatzzwecke, wie Crucibles, Boards und Quarzröhren zur Herstellung von Halbleitern eingesetzt werden, seitdem es möglich ist, dieses Kieselglas in hoher Reinheit herzustellen.silica glass can be beneficial for many uses, such as crucibles, boards and quartz tubes for Manufacture of semiconductors since it is possible to to produce this silica glass in high purity.

Weiterhin wird das Siliciumdioxidglas für die Glasgeräte in der Chemie oder für die Photozelle verwendet. Es kann zur Herstellung von Lichtleitfasern verwendet werden.Farther is the silica glass for the glassware in chemistry or for the photocell used. It can be used to manufacture optical fibers be used.

Es ist bekannt Siliciumdioxidglas zum Beispiel in Form eines Monolithen herzustellen, indem man Siliciumalkoxid hydrolysiert, pyrogene Kieselsäure zu der hydrolysierten Lösung hinzugibt, die Mischung zu einem Gel gellieren läßt, das Gel trocknet und das erhaltene trockne Gel sintert ( US 4,681,615 , US 4,801,318 ).It is known to prepare silica glass, for example in the form of a monolith, by hydrolyzing silicon alkoxide, adding fumed silica to the hydrolyzed solution, gelling the mixture to a gel, drying the gel and sintering the resultant dry gel ( US 4,681,615 . US 4,801,318 ).

Bei dem bekannten Verfahren können bekannte pyrogen hergestellte Siliciumdioxide eingesetzt werden.at the known method can known pyrogenic silicas are used.

Die bekannten pyrogenen Kieselsäuren weisen den Nachteil auf, daß sie für die besonders hohen Ansprüche an die Reinheit des Glases noch zu viele Fremdelemente enthalten.The known fumed silicas have the disadvantage that they for the particularly high standards to the purity of the glass still contain too many foreign elements.

Gegenstand der Erfindung ist ein hochreines, pyrogen hergestelltes Siliciumdioxid, welches gekennzeichnet ist durch einen Gehalt an Metallen von kleiner 9 ppm.object the invention is a high-purity, pyrogenic silica, which is characterized by a content of metals of smaller 9 ppm.

In einer bevorzugten Ausführungsform der Erfindung kann das hochreine pyrogen hergestellte Siliciumdioxid gekennzeichnet sein durch den folgenden Gehalt an Metallen:

Figure 00020001
In a preferred embodiment of the invention, the high purity pyrogenic silica may be characterized by the following metals content:
Figure 00020001

Der Gesamtmetallgehalt kann dann 3252 ppb (~ 3,2 ppm) oder kleiner betragen.Of the Total metal content may then be 3252 ppb (~ 3.2 ppm) or less.

In einer weiter bevorzugten Ausführungsform der Erfindung kann das hochreine pyrogen hergestellte Siliciumdioxid gekennzeichnet sein durch den folgenden Gehalt an Metallen:

Figure 00030001
In a further preferred embodiment of the invention, the high-purity pyrogenically prepared silicon dioxide may be characterized by the following content of metals:
Figure 00030001

Der Gesamtmetallgehalt kann dann 1033 ppb (~ 1,03 ppm) oder kleiner betragen.Of the Total metal content can then be 1033 ppb (~ 1.03 ppm) or less be.

Ein weiterer Gegenstand der Erfindung ist ein Verfahren zur Herstellung des hochreinen, pyrogen hergestellten Siliciumdioxides, welches dadurch gekennzeichnet ist, daß man Siliciumtetrachlorid auf bekannte Weise mittels Hochtemperaturhydrolyse zu Siliciumdioxid in der Flamme umsetzt und dabei ein Siliciumtetrachlorid verwendet, welches einen Metallgehalt von kleiner 30 ppb aufweist.One Another object of the invention is a process for the preparation of the highly pure, pyrogenically produced silicon dioxide, which characterized in that one Silicon tetrachloride in a known manner by means of high temperature hydrolysis converts to silica in the flame and thereby a silicon tetrachloride used, which has a metal content of less than 30 ppb.

In einer bevorzugten Ausführungsform der Erfindung kann man ein Siliciumtetrachlorid verwenden, welches neben Siliciumtetrachlorid den folgenden Gehalt an Metallen aufweist:

Figure 00040001
In a preferred embodiment of the invention, it is possible to use a silicon tetrachloride which, in addition to silicon tetrachloride, has the following content of metals:
Figure 00040001

Siliciumtetrachlorid mit diesem niedrigen Metallgehalt kann gemäß DE 100 30 251 oder gemäß DE 100 30 252 hergestellt werden.Silicon tetrachloride with this low metal content can be prepared according to DE 100 30 251 or according to DE 100 30 252 getting produced.

Das prinzipielle Verfahren zur Herstellung von pyrogenem Siliciumdioxid, ausgehend von Siliciumtetrachlorid, das im Gemisch mit Wasserstoff und Sauerstoff umgesetzt wird, ist bekannt aus Ullmanns Enzyklopädie der technischen Chemie, 4. Auflage, Band 21, Seite 464 ff. (1982).The Principal processes for the preparation of fumed silica, starting from silicon tetrachloride mixed with hydrogen and oxygen is converted, is known from Ullmanns encyclopedia of Technical Chemistry, 4th Edition, Volume 21, page 464 ff. (1982).

Metallgehalt des erfindungsgemäßen Siliciumdioxides liegt im ppm-Bereich und darunter (ppb-Bereich).metal content of the silicon dioxide according to the invention is in the ppm range and below (ppb range).

Das erfindungsgemäße pyrogen hergestellte Siliciumdioxid kann bei den verschiedensten Glasherstellungsmethoden, wie zum Beispiel dem Sol-Gel-Verfahren eingesetzt werden. Derartige Sol-Gel-Verfahren sind bekannt aus US 4,681,615 oder US 4,801,318 .The pyrogenically prepared silicon dioxide according to the invention can be used in a wide variety of glass production methods, for example the sol-gel method. Such sol-gel methods are known from US 4,681,615 or US 4,801,318 ,

Das erfindungsgemäße pyrogen hergestellte Siliciumdioxid eignet sich vorteilhaft zur Herstellung von Spezialgläsern mit hervorragenden optischen Eigenschaften.The pyrogen according to the invention produced silica is advantageously suitable for the preparation of special glasses with excellent optical properties.

Die mittels dem erfindungsgemäßen Siliciumdioxid hergestellten Gläser weisen eine besonders geringe Adsorption im tiefen UV-Bereich auf.The by means of the silica according to the invention produced glasses have a particularly low adsorption in the deep UV range.

Beispiel 1 (Vergleichsbeispiel) Example 1 (comparative example)

500 kg/h SiCl4 einer Zusammensetzung gemäß Tabelle 1 werden bei ca. 90 °C verdampft und in das Zentralrohr eines Brenners bekannter Bauart überführt. In dieses Rohr werden zusätzlich 190 Nm3/h Wasserstoff sowie 326 Nm3/h Luft mit einem Sauerstoffanteil von 35 Vol% gegeben. Dieses Gasgemisch wird entzündet und brennt im Flammrohr des wassergekühlten Brenners. In eine die Zentraldüse umgebende Manteldüse werden zur Vermeidung von Anbackungen zusätzlich 15 Nm3/h Wasserstoff gegeben. In das Flammrohr wird außerdem zusätzlich 250 Nm3/h Luft normaler Zusammensetzung gegeben. Nach der Abkühlung der Reaktionsgase wird das pyrogene Siliciumdioxidpulver von den salzsäurehaltigen Gasen mittels eines Filters und/oder eines Zyklons abgetrennt. In einer Entsäuerungseinheit wird das pyrogene Siliciumdioxidpulver mit Wasserdampf und Luft behandelt, um es von anhaftender Salzsäure zu befreien. Die Metallgehalte sind in der Tabelle 3 wiedergegeben.500 kg / h SiCl 4 of a composition shown in Table 1 are evaporated at about 90 ° C and transferred to the central tube of a burner of known design. In addition, 190 Nm 3 / h of hydrogen and 326 Nm 3 / h of air with an oxygen content of 35% by volume are added to this tube. This gas mixture is ignited and burns in the flame tube of the water-cooled burner. In a surrounding the central nozzle jacket nozzle to prevent caking additionally 15 Nm 3 / h of hydrogen. In addition, 250 Nm 3 / h of air of normal composition are added to the flame tube. After cooling of the reaction gases, the fumed silica powder is separated from the hydrochloric acid-containing gases by means of a filter and / or a cyclone. In a deacidification unit, the fumed silica powder is treated with water vapor and air to remove adherent hydrochloric acid. The metal contents are shown in Table 3.

Beispiel 2 (Ausführungsbeispiel)Example 2 (embodiment)

500 kg/h SiCl4 einer Zusammensetzung gemäß Tabelle 2 werden bei ca. 90 °C verdampft und in das Zentralrohr eines Brenners bekannter Bauart überführt. In dieses Rohr werden zusätzlich 190 Nm3/h Wasserstoff sowie 326 Nm3/h Luft mit einem Sauerstoffanteil von 35 Vol% gegeben. Dieses Gasgemisch wird entzündet und brennt im Flammrohr des wassergekühlten Brenners. In eine die Zentraldüse umgebende Manteldüse werden zur Vermeidung von Anbackungen zusätzlich 15 Nm3/h Wasserstoff gegeben. In das Flammrohr wird außerdem zusätzlich 250 Nm3/h Luft normaler Zusammensetzung gegeben. Nach der Abkühlung der Reaktionsgase wird das pyrogene Siliciumdioxidpulver von den salzsäurehaltigen Gasen mittels eines Filters und/oder eines Zyklons abgetrennt. In einer Entsäuerungseinheit wird das pyrogene Siliciumdioxidpulver mit Wasserdampf und Luft behandelt, um es von anhaftender Salzsäure zu befreien.500 kg / h SiCl 4 of a composition according to Table 2 are evaporated at about 90 ° C and transferred to the central tube of a burner of known design. In addition, 190 Nm 3 / h of hydrogen and 326 Nm 3 / h of air with an oxygen content of 35% by volume are added to this tube. This gas mixture is ignited and burns in the flame tube of the water-cooled burner. In a surrounding the central nozzle jacket nozzle to prevent caking additionally 15 Nm 3 / h of hydrogen. In addition, 250 Nm 3 / h of air of normal composition are added to the flame tube. After cooling of the reaction gases, the fumed silica powder is separated from the hydrochloric acid-containing gases by means of a filter and / or a cyclone. In a deacidification unit, the fumed silica powder is treated with water vapor and air to remove adherent hydrochloric acid.

Die Metallgehalte sind in der Tabelle 3 wiedergegeben.The Metal contents are given in Table 3.

Tabelle 1: Zusammensetzung SiCl4, Beispiel 1

Figure 00070001
Table 1: Composition SiCl 4 , Example 1
Figure 00070001

Tabelle 2: Zusammensetzung SiCl4, Beispiel 2

Figure 00070002
Table 2: Composition SiCl 4 , Example 2
Figure 00070002

Figure 00080001
Figure 00080001

MeßmethodeMeasurement Method

Die erhaltenen pyrogen hergestellten Siliciumdioxide werden in Bezug auf ihren Metallgehalt analysiert. Die Proben werden in einer Säurelösung, die hauptsächlich aus HF besteht, gelöst.The obtained pyrogenic silicas are obtained in relation analyzed for their metal content. The samples are dissolved in an acid solution, the mainly consists of HF, solved.

Das SiO2 reagiert mit dem HF und bildet SiF4 + H2O. Das SiF4 verdampft und läßt die zu bestimmenden Metalle vollständig in der Säure zurück. Die einzelnen Proben werden mit destilliertem Wasser verdünnt und mittels der Perkin Elmer Optima 3000 DV Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) gegen einen internen Standard analysiert. Die Ungenauigkeit der Werte rührt von Proben-Affekten, Spektral Interferencen und der Begrenztheit der Meßmethode her. Größere Elemente haben eine relative Ungenauigkeit von ± 5 %, während die kleineren Elemente eine relative Ungenauigkeit von ± 15 % aufweisen.The SiO 2 reacts with the HF and forms SiF 4 + H 2 O. The SiF 4 evaporates and leaves the metals to be determined completely in the acid. The individual samples are diluted with distilled water and analyzed against an internal standard using the Perkin Elmer Optima 3000 DV Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES). The inaccuracy of the values is due to sample affects, spectral interferences, and the limitations of the method of measurement. Larger elements have a relative inaccuracy of ± 5%, while the smaller elements have a relative inaccuracy of ± 15%.

Claims (6)

Hochreines, pyrogen hergestelltes Siliciumdioxid, gekennzeichnet durch einen Gehalt an Metallen von kleiner 9 ppm.High purity fumed silica, characterized by a content of metals of less than 9 ppm. Hochreines, pyrogen hergestelltes Siliciumdioxid gemäß Anspruch 1, gekennzeichnet durch den folgenden Gehalt der Metalle:
Figure 00100001
High-purity, pyrogenically produced silicon dioxide according to claim 1, characterized by the following content of the metals:
Figure 00100001
 Verfahren zur Herstellung des hochreinen, pyrogen hergestellten Siliciumdioxides gemäß den Ansprüchen 1 oder 2, dadurch gekennzeichnet, daß man Siliciumtetrachlorid auf bekannte Weise mittels Hochtemperaturhydrolyse zu Siliciumdioxid in der Flamme umsetzt und dabei ein Siliciumtetrachlorid verwendet, welches einen Metallgehalt von kleiner 30 ppb aufweist.Process for the preparation of high purity, pyrogenic produced silicon dioxide according to claims 1 or 2, characterized in that that is silicon tetrachloride in a known manner by means of high-temperature hydrolysis to silica reacted in the flame using a silicon tetrachloride, which has a metal content of less than 30 ppb. Verfahren zur Herstellung des hochreinen, pyrogen hergestellten Siliciumdioxides gemäß Anspruch 3, dadurch gekennzeichnet, daß man Siliciumtetrachlorid auf bekannter Waise mittels Hochtemperaturhydrolyse zu Siliciumdioxid in der Flamme umsetzt und dabei ein Siliciumtetrachlorid verwendet, welches neben Siliciumtetrachlorid den folgenden Gehalt an Metallen aufweist:
Figure 00110001
Process for the preparation of the high-purity pyrogenically prepared silicon dioxide according to Claim 3, characterized in that silicon tetrachloride is known on orphan by means of high-temperature hydrolysis converts to silica in the flame and thereby uses a silicon tetrachloride, which in addition to silicon tetrachloride has the following content of metals:
Figure 00110001
 Verwendung des hochreinen, pyrogen hergestellten Siliciumdioxides gemäß Anspruch 1 zur Herstellung von Gläsern.Use of high purity, pyrogenic Silica according to claim 1 for the production of glasses. Verwendung des hochreinen, pyrogen hergestellten Siliciumdioxides gemäß Anspruch 5 zur Herstellung von Gläsern mittels dem Sol-Gel-Verfahren.Use of high purity, pyrogenic Silica according to claim 5 for the production of glasses by the sol-gel method.
DE10342828A 2003-09-17 2003-09-17 High purity pyrogenic silica Withdrawn DE10342828A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
DE10342828A DE10342828A1 (en) 2003-09-17 2003-09-17 High purity pyrogenic silica
JP2006526581A JP4903045B2 (en) 2003-09-17 2004-09-16 High purity silicon dioxide produced by pyrolysis
PCT/EP2004/010335 WO2005026068A2 (en) 2003-09-17 2004-09-16 High-purity pyrogenically prepared silicon dioxide
CNA2004800268452A CN1863733A (en) 2003-09-17 2004-09-16 High-purity pyrogenically prepared silicon dioxide
KR1020067005468A KR100789124B1 (en) 2003-09-17 2004-09-16 A high-purity pyrogenically prepared silicon dioxide, a process for the preparation of the same, and a silica glass and articles obtained by using the same
EP04786950A EP1663888A2 (en) 2003-09-17 2004-09-16 High-purity pyrogenically prepared silicon dioxide
US10/571,332 US20070003770A1 (en) 2003-09-17 2004-09-16 High-purity pyrogenically prepared silicon dioxide

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KR (1) KR100789124B1 (en)
CN (1) CN1863733A (en)
DE (1) DE10342828A1 (en)
WO (1) WO2005026068A2 (en)

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EP1700830A1 (en) 2005-03-09 2006-09-13 Novara Technology S.R.L. Process for the production of monoliths by means of the invert sol-gel process
EP1700831A1 (en) 2005-03-09 2006-09-13 Novara Technology S.R.L. Process for the production of monoliths by means of the sol-gel process
EP1700829A1 (en) 2005-03-09 2006-09-13 Degussa AG Process for the production of glass-monoliths by means of the sol-gel process

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EP1663888A2 (en) 2006-06-07
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US20070003770A1 (en) 2007-01-04

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